气相色谱-质谱联用法检测干红菇中5种农药残留量

Determination of 5 kinds of pesticide residues in dried Russula by gas chromatography-mass spectrometry

中文关键词:  红菇  气相色谱-质谱联用法  农药残留

英文关键词:Russula  gas chromatography-mass spectrometry  pesticide residues

中文摘要:

      目的 建立气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)测定干红菇中5种农药(灭线磷、甲拌磷、氯唑磷、水胺硫磷、哒螨灵)残留量的分析方法。方法 样品用乙腈提取, 过商品化固相萃取柱(solid phase extraction column, SPE)净化浓缩, 正己烷定容, 在气相色谱-质谱系统的单离子扫描(single ion monitoring, SIM)模式下, 对5种农药进行定性和定量分析。结果 5种农药在0.01~2.0 mg/L的范围内呈现良好线性关系, 相关系数r2均大于0.995; 方法的检出限和定量限分别为0.003~0.010 mg/kg和0.009~ 0.033 mg/kg; 在3个加标水平下(0.05、0.1、0.5 mg/kg), 加标回收率为75.9%~96.7%, 相对标准偏差(relative standard deviation, RSD)为1.60%~8.57%。结论 本方法的重复性和回收率满足实验要求, 适用干红菇中部分农药残留的分析检测。

英文摘要:

      Objective To establish a method for the determination of 5 kinds of pesticide residues (ethoprophos, phorate, isazofos, isocarbophos, and pyridaben) in dried Russula by gas chromatography-mass spectrometry (GC-MS). Methods The samples were extracted with acetonitrile, purified and concentrated with a solid phase extraction column (SPE), and volume-stabilized with n-hexane. In the single ion monitoring (SIM) mode of the gas chromatography-mass spectrometry system, qualitative and quantitative analysis of 5 pesticides were performed. Results All the 5 pesticide residues showed good linear relationships in the range of 0.01?2.0 mg/L, while the correlation coefficients r2 were greater than 0.995. The limits of detection and limits of quantitative were 0.003? 0.010 mg/kg and 0.009?0.033 mg/kg, respectively. At the standard addition levels of 0.05, 0.1 and 0.5 mg/kg, the standard addition recoveries were 75.9%?96.7%, and the relative standard deviations (RSDs) were 1.60%?8.57%. Conclusion The repeatability and recovery of the method can meet the experimental requirements, and the method is applicable for the detection and analysis of part of pesticide residues in dried Russula.